data_JMWPD176 _audit_creation_method SHELXL-97_chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H39 B2 Cu F8 N14' _chemical_formula_weight 892.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.537(5) _cell_length_b 12.735(5) _cell_length_c 14.852(5) _cell_angle_alpha 108.124(5) _cell_angle_beta 103.591(5) _cell_angle_gamma 106.069(5) _cell_volume 2027.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 130.00(10) _cell_measurement_reflns_used 9195 _cell_measurement_theta_min 2.8735 _cell_measurement_theta_max 29.2094 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_F_000 916 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.4154 _exptl_crystal_size_mid 0.2722 _exptl_crystal_size_min 0.1278 _exptl_absorpt_coefficient_mu 0.622 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130.00(10) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17327 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.880 _diffrn_reflns_theta_max 24.996 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.970 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.970 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.970 _reflns_number_total 7112 _reflns_number_gt 6304 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+8.2959P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7112 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4602(4) 0.2541(4) 0.2083(3) 0.0222(9) Uani 1 1 d . . . . . H1A H 0.4370 0.3151 0.1932 0.027 Uiso 1 1 calc R U . . . H1B H 0.3891 0.1886 0.1959 0.027 Uiso 1 1 calc R U . . . C2 C 0.5255(4) 0.2108(4) 0.1422(3) 0.0201(9) Uani 1 1 d . . . . . C3 C 0.6563(4) 0.1502(4) 0.0966(3) 0.0220(9) Uani 1 1 d . . . . . C4 C 0.7539(4) 0.1183(4) 0.0907(4) 0.0256(10) Uani 1 1 d . . . . . H4 H 0.8090 0.1231 0.1476 0.031 Uiso 1 1 calc R U . . . C5 C 0.7640(4) 0.0794(4) -0.0034(4) 0.0285(11) Uani 1 1 d . . . . . H5 H 0.8285 0.0591 -0.0095 0.034 Uiso 1 1 calc R U . . . C6 C 0.6813(4) 0.0695(4) -0.0892(4) 0.0284(11) Uani 1 1 d . . . . . H6 H 0.6912 0.0420 -0.1513 0.034 Uiso 1 1 calc R U . . . C7 C 0.5842(4) 0.0998(4) -0.0845(4) 0.0272(10) Uani 1 1 d . . . . . H7 H 0.5286 0.0936 -0.1417 0.033 Uiso 1 1 calc R U . . . C8 C 0.5744(4) 0.1396(4) 0.0101(4) 0.0240(10) Uani 1 1 d . . . . . C9 C 0.4677(4) 0.2846(4) 0.3811(3) 0.0191(9) Uani 1 1 d . . . . . H9A H 0.5113 0.3423 0.4505 0.023 Uiso 1 1 calc R U . . . H9B H 0.3933 0.2939 0.3576 0.023 Uiso 1 1 calc R U . . . C10 C 0.4454(4) 0.1610(4) 0.3751(3) 0.0194(9) Uani 1 1 d . . . . . C11 C 0.4735(4) -0.0030(4) 0.3584(3) 0.0203(9) Uani 1 1 d . . . . . C12 C 0.5136(4) -0.0969(4) 0.3426(4) 0.0247(10) Uani 1 1 d . . . . . H12 H 0.5781 -0.0945 0.3214 0.030 Uiso 1 1 calc R U . . . C13 C 0.4537(4) -0.1933(4) 0.3595(4) 0.0265(10) Uani 1 1 d . . . . . H13 H 0.4786 -0.2570 0.3496 0.032 Uiso 1 1 calc R U . . . C14 C 0.3564(5) -0.1977(4) 0.3911(4) 0.0301(11) Uani 1 1 d . . . . . H14 H 0.3180 -0.2644 0.4015 0.036 Uiso 1 1 calc R U . . . C16 C 0.3757(4) -0.0091(4) 0.3890(3) 0.0211(9) Uani 1 1 d . . . . . C17 C 0.6128(4) 0.4326(4) 0.3514(3) 0.0211(9) Uani 1 1 d . . . . . H17A H 0.5700 0.4816 0.3752 0.025 Uiso 1 1 calc R U . . . H17B H 0.6336 0.4490 0.2969 0.025 Uiso 1 1 calc R U . . . C18 C 0.7225(4) 0.4593(4) 0.4361(3) 0.0197(9) Uani 1 1 d . . . . . C19 C 0.8636(4) 0.4278(4) 0.5255(3) 0.0190(9) Uani 1 1 d . . . . . C20 C 0.9411(4) 0.3817(4) 0.5665(3) 0.0220(9) Uani 1 1 d . . . . . H20 H 0.9267 0.3007 0.5387 0.026 Uiso 1 1 calc R U . . . C21 C 1.0405(4) 0.4608(4) 0.6502(4) 0.0248(10) Uani 1 1 d . . . . . H21 H 1.0939 0.4323 0.6794 0.030 Uiso 1 1 calc R U . . . C22 C 1.0624(4) 0.5828(4) 0.6917(4) 0.0265(10) Uani 1 1 d . . . . . H22 H 1.1307 0.6336 0.7475 0.032 Uiso 1 1 calc R U . . . C23 C 0.9861(4) 0.6295(4) 0.6525(4) 0.0259(10) Uani 1 1 d . . . . . H23 H 1.0003 0.7105 0.6809 0.031 Uiso 1 1 calc R U . . . C24 C 0.8862(4) 0.5498(4) 0.5681(3) 0.0210(9) Uani 1 1 d . . . . . C25 C 0.8276(4) 0.0853(4) 0.3429(4) 0.0233(10) Uani 1 1 d . . . . . C26 C 0.9156(5) 0.0319(5) 0.3500(5) 0.0368(12) Uani 1 1 d . . . . . H26A H 0.9650 0.0542 0.3132 0.055 Uiso 1 1 calc R U . . . H26B H 0.8766 -0.0534 0.3218 0.055 Uiso 1 1 calc R U . . . H26C H 0.9635 0.0595 0.4198 0.055 Uiso 1 1 calc R U . . . C27 C 1.1864(7) 0.1706(6) 0.9416(5) 0.0578(19) Uani 1 1 d . . . . . C28 C 1.0887(7) 0.1844(7) 0.9744(5) 0.067(2) Uani 1 1 d . . . . . H28A H 1.0870 0.2614 0.9818 0.100 Uiso 1 1 calc R U . . . H28B H 1.0993 0.1774 1.0381 0.100 Uiso 1 1 calc R U . . . H28C H 1.0153 0.1234 0.9249 0.100 Uiso 1 1 calc R U . . . C29 C 1.1856(7) 0.5974(7) 0.9769(6) 0.067(2) Uani 1 1 d . . . . . H29A H 1.1959 0.6796 0.9935 0.101 Uiso 1 1 calc R U . . . H29B H 1.2148 0.5866 1.0378 0.101 Uiso 1 1 calc R U . . . H29C H 1.1029 0.5479 0.9428 0.101 Uiso 1 1 calc R U . . . C30 C 1.2515(5) 0.5641(6) 0.9107(5) 0.0436(14) Uani 1 1 d . . . . . C31 C 1.5302(7) 0.6401(6) 1.1213(5) 0.0602(18) Uani 1 1 d . . . . . H31A H 1.5324 0.6325 1.0554 0.090 Uiso 1 1 calc R U . . . H31B H 1.6076 0.6558 1.1652 0.090 Uiso 1 1 calc R U . . . H31C H 1.5062 0.7048 1.1485 0.090 Uiso 1 1 calc R U . . . C32 C 1.4485(6) 0.5330(6) 1.1134(5) 0.0485(15) Uani 1 1 d . . . . . C33 C 0.9983(7) 0.2078(6) 0.7314(5) 0.0563(17) Uani 1 1 d . . . . . H33A H 1.0807 0.2256 0.7640 0.084 Uiso 1 1 calc R U . . . H33B H 0.9872 0.2194 0.6695 0.084 Uiso 1 1 calc R U . . . H33C H 0.9528 0.1264 0.7168 0.084 Uiso 1 1 calc R U . . . C34 C 0.9594(6) 0.2861(6) 0.7974(5) 0.0485(15) Uani 1 1 d . . . . . C35 C 0.8080(6) -0.4684(8) 0.7778(5) 0.0619(19) Uani 1 1 d . . . . . H35A H 0.7932 -0.5322 0.8003 0.093 Uiso 1 1 calc R U . . . H35B H 0.8261 -0.3945 0.8330 0.093 Uiso 1 1 calc R U . . . H35C H 0.8738 -0.4631 0.7546 0.093 Uiso 1 1 calc R U . . . C36 C 0.7041(5) -0.4912(5) 0.6962(5) 0.0366(12) Uani 1 1 d . . . . . C15 N 0.3161(5) -0.1056(4) 0.4073(4) 0.0433(11) Uani 1 1 d . . . . . H15 H 0.2571 -0.1077 0.4276 0.052 Uiso 1 1 calc R U . . . N1 N 0.5386(3) 0.3040(3) 0.3154(3) 0.0188(8) Uani 1 1 d . . . . . N2 N 0.3610(3) 0.0972(3) 0.3985(3) 0.0219(8) Uani 1 1 d . . . . . N3 N 0.5159(3) 0.1061(3) 0.3500(3) 0.0195(8) Uani 1 1 d . . . . . N4 N 0.4920(4) 0.1798(3) 0.0433(3) 0.0224(8) Uani 1 1 d . . . . . N5 N 0.6235(3) 0.1946(3) 0.1799(3) 0.0199(8) Uani 1 1 d . . . . . N6 N 0.7583(3) 0.3729(3) 0.4424(3) 0.0192(8) Uani 1 1 d . . . . . N7 N 0.7939(3) 0.5650(3) 0.5087(3) 0.0213(8) Uani 1 1 d . . . . . N8 N 0.7598(3) 0.1278(3) 0.3369(3) 0.0255(9) Uani 1 1 d . . . . . N9 N 1.2640(6) 0.1619(6) 0.9163(5) 0.0701(18) Uani 1 1 d . . . . . N10 N 1.3005(5) 0.5365(6) 0.8586(4) 0.0574(14) Uani 1 1 d . . . . . N11 N 1.3798(7) 0.4443(7) 1.1045(6) 0.077(2) Uani 1 1 d . . . . . N12 N 0.6238(4) -0.5113(4) 0.6316(4) 0.0392(11) Uani 1 1 d . . . . . N13 N 0.9316(6) 0.3488(6) 0.8519(5) 0.0708(18) Uani 1 1 d . . . . . F1 F 0.6964(3) -0.2785(2) 0.4495(2) 0.0328(7) Uani 1 1 d . . . . . F2 F 0.8802(3) -0.2258(3) 0.4392(3) 0.0440(8) Uani 1 1 d . . . . . F3 F 0.8082(3) -0.0838(2) 0.4974(2) 0.0348(7) Uani 1 1 d . . . . . F4 F 0.7307(3) -0.2079(3) 0.3322(2) 0.0501(9) Uani 1 1 d . . . . . F6 F 0.9856(2) -0.1117(3) 0.8167(2) 0.0395(7) Uani 1 1 d . . . . . F5 F 0.7980(7) -0.197(3) 0.8051(12) 0.074(6) Uani 0.71(5) 1 d . . P A 1 F7 F 0.854(2) -0.0230(16) 0.7877(11) 0.077(6) Uani 0.71(5) 1 d . . P A 1 F5' F 0.804(2) -0.140(3) 0.8231(19) 0.065(7) Uani 0.29(5) 1 d . . P A 2 F7' F 0.891(3) -0.016(3) 0.769(3) 0.065(8) Uani 0.29(5) 1 d . . P A 2 F8 F 0.8325(3) -0.1945(3) 0.6669(2) 0.0404(8) Uani 1 1 d . . . . . Cu Cu 0.65181(5) 0.21338(5) 0.32676(4) 0.01985(19) Uani 1 1 d . . . . . B1 B 0.7789(5) -0.1996(5) 0.4282(4) 0.0296(12) Uani 1 1 d . . . . . B2 B 0.8701(5) -0.1285(6) 0.7693(4) 0.0308(13) Uani 1 1 d . . . . . H2A H 0.322(5) 0.119(5) 0.419(4) 0.018(14) Uiso 1 1 d . . . . . H4A H 0.438(5) 0.185(4) 0.012(4) 0.018(13) Uiso 1 1 d . . . . . H7A H 0.780(5) 0.619(5) 0.507(4) 0.025(14) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(2) 0.026(2) 0.027(2) 0.010(2) 0.0071(19) 0.0103(19) C2 0.016(2) 0.018(2) 0.025(2) 0.0086(18) 0.0071(18) 0.0046(18) C3 0.018(2) 0.020(2) 0.024(2) 0.0053(19) 0.0095(19) 0.0046(18) C4 0.020(2) 0.025(2) 0.027(2) 0.004(2) 0.009(2) 0.008(2) C5 0.023(2) 0.029(3) 0.033(3) 0.007(2) 0.015(2) 0.011(2) C6 0.030(3) 0.025(2) 0.024(2) 0.003(2) 0.014(2) 0.007(2) C7 0.027(2) 0.025(2) 0.022(2) 0.005(2) 0.007(2) 0.005(2) C8 0.020(2) 0.021(2) 0.028(2) 0.0075(19) 0.010(2) 0.0045(19) C9 0.016(2) 0.019(2) 0.025(2) 0.0067(18) 0.0097(18) 0.0092(18) C10 0.017(2) 0.018(2) 0.021(2) 0.0047(18) 0.0056(18) 0.0062(18) C11 0.017(2) 0.017(2) 0.021(2) 0.0034(18) 0.0026(18) 0.0049(18) C12 0.023(2) 0.021(2) 0.029(2) 0.007(2) 0.009(2) 0.011(2) C13 0.030(3) 0.021(2) 0.026(2) 0.006(2) 0.007(2) 0.012(2) C14 0.034(3) 0.022(2) 0.033(3) 0.011(2) 0.012(2) 0.009(2) C16 0.021(2) 0.019(2) 0.021(2) 0.0048(18) 0.0064(18) 0.0077(18) C17 0.021(2) 0.016(2) 0.027(2) 0.0067(18) 0.0089(19) 0.0088(18) C18 0.018(2) 0.019(2) 0.026(2) 0.0106(19) 0.0117(19) 0.0081(18) C19 0.015(2) 0.018(2) 0.023(2) 0.0055(18) 0.0090(18) 0.0053(17) C20 0.020(2) 0.017(2) 0.027(2) 0.0060(19) 0.0090(19) 0.0072(18) C21 0.020(2) 0.026(2) 0.029(2) 0.010(2) 0.009(2) 0.010(2) C22 0.017(2) 0.027(2) 0.028(3) 0.006(2) 0.007(2) 0.0035(19) C23 0.022(2) 0.018(2) 0.033(3) 0.006(2) 0.012(2) 0.0031(19) C24 0.017(2) 0.017(2) 0.028(2) 0.0065(19) 0.0116(19) 0.0054(18) C25 0.019(2) 0.018(2) 0.030(3) 0.0060(19) 0.009(2) 0.0068(19) C26 0.032(3) 0.043(3) 0.057(4) 0.029(3) 0.026(3) 0.025(3) C27 0.053(4) 0.046(4) 0.049(4) 0.021(3) -0.016(3) 0.009(3) C28 0.067(5) 0.075(5) 0.043(4) 0.017(4) 0.005(4) 0.026(4) C29 0.071(5) 0.064(5) 0.069(5) 0.021(4) 0.038(4) 0.023(4) C30 0.039(3) 0.045(3) 0.043(3) 0.020(3) 0.011(3) 0.012(3) C31 0.078(5) 0.044(4) 0.045(4) 0.009(3) 0.012(4) 0.022(4) C32 0.063(4) 0.060(4) 0.040(3) 0.027(3) 0.027(3) 0.033(4) C33 0.069(5) 0.062(4) 0.050(4) 0.023(3) 0.023(3) 0.041(4) C34 0.055(4) 0.051(4) 0.047(4) 0.022(3) 0.018(3) 0.028(3) C35 0.040(4) 0.101(6) 0.053(4) 0.042(4) 0.016(3) 0.027(4) C36 0.034(3) 0.040(3) 0.046(3) 0.025(3) 0.019(3) 0.016(3) C15 0.045(3) 0.036(3) 0.045(3) 0.012(2) 0.019(2) 0.013(2) N1 0.0146(17) 0.0177(18) 0.0244(19) 0.0069(15) 0.0092(15) 0.0064(15) N2 0.0189(19) 0.022(2) 0.029(2) 0.0084(17) 0.0142(18) 0.0118(17) N3 0.0172(18) 0.0164(18) 0.0227(19) 0.0047(15) 0.0064(15) 0.0072(15) N4 0.0149(19) 0.025(2) 0.025(2) 0.0087(17) 0.0049(17) 0.0083(17) N5 0.0142(17) 0.0206(19) 0.0226(19) 0.0064(15) 0.0072(15) 0.0053(15) N6 0.0153(18) 0.0187(18) 0.0234(19) 0.0067(15) 0.0068(15) 0.0078(15) N7 0.0181(19) 0.0146(19) 0.032(2) 0.0079(17) 0.0114(17) 0.0072(16) N8 0.023(2) 0.0181(19) 0.031(2) 0.0038(17) 0.0096(17) 0.0079(17) N9 0.040(3) 0.082(5) 0.092(5) 0.048(4) 0.005(3) 0.027(3) N10 0.055(3) 0.068(4) 0.050(3) 0.026(3) 0.015(3) 0.025(3) N11 0.098(5) 0.078(5) 0.090(5) 0.053(4) 0.057(4) 0.042(4) N12 0.034(3) 0.040(3) 0.054(3) 0.022(2) 0.022(3) 0.021(2) N13 0.080(5) 0.072(4) 0.066(4) 0.017(3) 0.031(4) 0.043(4) F1 0.0308(15) 0.0291(15) 0.0430(17) 0.0160(13) 0.0157(13) 0.0138(13) F2 0.0406(18) 0.0445(19) 0.062(2) 0.0205(17) 0.0314(17) 0.0284(16) F3 0.0369(16) 0.0259(15) 0.0463(18) 0.0108(13) 0.0245(14) 0.0144(13) F4 0.066(2) 0.048(2) 0.0350(18) 0.0188(16) 0.0152(17) 0.0193(18) F6 0.0184(14) 0.0494(19) 0.0424(18) 0.0104(15) 0.0061(13) 0.0141(14) F5 0.025(3) 0.141(15) 0.050(6) 0.066(7) 0.005(3) 0.000(5) F7 0.082(10) 0.063(7) 0.052(5) -0.019(4) -0.021(5) 0.063(8) F5' 0.032(9) 0.066(16) 0.096(16) 0.014(11) 0.048(11) 0.017(9) F7' 0.041(11) 0.051(12) 0.099(19) 0.019(12) 0.023(11) 0.024(9) F8 0.0314(16) 0.0465(19) 0.0321(16) 0.0013(14) 0.0072(13) 0.0185(15) Cu 0.0161(3) 0.0182(3) 0.0258(3) 0.0059(2) 0.0081(2) 0.0099(2) B1 0.035(3) 0.028(3) 0.035(3) 0.014(3) 0.020(3) 0.017(3) B2 0.021(3) 0.043(3) 0.031(3) 0.014(3) 0.010(2) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.481(6) . ? C1 C2 1.492(6) . ? C2 N5 1.323(6) . ? C2 N4 1.323(6) . ? C3 C8 1.385(7) . ? C3 N5 1.398(6) . ? C3 C4 1.404(6) . ? C4 C5 1.379(7) . ? C5 C6 1.387(7) . ? C6 C7 1.385(7) . ? C7 C8 1.385(7) . ? C8 N4 1.395(6) . ? C9 C10 1.491(6) . ? C9 N1 1.496(5) . ? C10 N3 1.320(6) . ? C10 N2 1.331(6) . ? C11 C12 1.396(6) . ? C11 C16 1.396(6) . ? C11 N3 1.399(6) . ? C12 C13 1.381(7) . ? C13 C14 1.400(7) . ? C14 C15 1.378(7) . ? C16 N2 1.386(6) . ? C16 C15 1.391(7) . ? C17 N1 1.488(6) . ? C17 C18 1.500(6) . ? C18 N6 1.318(6) . ? C18 N7 1.324(6) . ? C19 C20 1.385(6) . ? C19 N6 1.394(6) . ? C19 C24 1.398(6) . ? C20 C21 1.383(7) . ? C21 C22 1.400(7) . ? C22 C23 1.371(7) . ? C23 C24 1.392(7) . ? C24 N7 1.380(6) . ? C25 N8 1.129(6) . ? C25 C26 1.447(6) . ? C27 N9 1.144(10) . ? C27 C28 1.453(12) . ? C29 C30 1.465(9) . ? C30 N10 1.128(8) . ? C31 C32 1.412(10) . ? C32 N11 1.163(9) . ? C33 C34 1.441(9) . ? C34 N13 1.140(8) . ? C35 C36 1.442(9) . ? C36 N12 1.118(7) . ? N1 Cu 2.070(4) . ? N3 Cu 2.042(4) . ? N5 Cu 2.051(4) . ? N6 Cu 2.027(4) . ? N8 Cu 1.966(4) . ? F1 B1 1.397(6) . ? F2 B1 1.385(6) . ? F3 B1 1.395(6) . ? F4 B1 1.370(7) . ? F6 B2 1.377(6) . ? F5 B2 1.396(12) . ? F7 B2 1.365(14) . ? F5' B2 1.29(3) . ? F7' B2 1.39(4) . ? F8 B2 1.375(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 108.8(3) . . ? N5 C2 N4 113.3(4) . . ? N5 C2 C1 120.9(4) . . ? N4 C2 C1 125.8(4) . . ? C8 C3 N5 109.4(4) . . ? C8 C3 C4 120.2(4) . . ? N5 C3 C4 130.4(4) . . ? C5 C4 C3 116.8(4) . . ? C4 C5 C6 122.3(4) . . ? C7 C6 C5 121.4(4) . . ? C8 C7 C6 116.4(4) . . ? C7 C8 C3 122.9(4) . . ? C7 C8 N4 132.1(5) . . ? C3 C8 N4 104.9(4) . . ? C10 C9 N1 107.2(3) . . ? N3 C10 N2 113.0(4) . . ? N3 C10 C9 120.9(4) . . ? N2 C10 C9 126.1(4) . . ? C12 C11 C16 120.2(4) . . ? C12 C11 N3 131.1(4) . . ? C16 C11 N3 108.7(4) . . ? C13 C12 C11 117.4(4) . . ? C12 C13 C14 121.7(4) . . ? C15 C14 C13 121.5(5) . . ? N2 C16 C15 132.2(4) . . ? N2 C16 C11 105.3(4) . . ? C15 C16 C11 122.4(4) . . ? N1 C17 C18 107.0(3) . . ? N6 C18 N7 112.9(4) . . ? N6 C18 C17 120.2(4) . . ? N7 C18 C17 126.9(4) . . ? C20 C19 N6 131.2(4) . . ? C20 C19 C24 120.7(4) . . ? N6 C19 C24 108.1(4) . . ? C21 C20 C19 117.4(4) . . ? C20 C21 C22 121.3(4) . . ? C23 C22 C21 121.9(4) . . ? C22 C23 C24 116.7(4) . . ? N7 C24 C23 132.5(4) . . ? N7 C24 C19 105.6(4) . . ? C23 C24 C19 122.0(4) . . ? N8 C25 C26 179.2(5) . . ? N9 C27 C28 178.8(8) . . ? N10 C30 C29 178.7(8) . . ? N11 C32 C31 178.4(8) . . ? N13 C34 C33 178.0(8) . . ? N12 C36 C35 178.3(7) . . ? C14 C15 C16 116.7(4) . . ? C1 N1 C17 111.5(3) . . ? C1 N1 C9 110.7(3) . . ? C17 N1 C9 111.1(3) . . ? C1 N1 Cu 108.3(2) . . ? C17 N1 Cu 107.7(2) . . ? C9 N1 Cu 107.4(3) . . ? C10 N2 C16 107.7(4) . . ? C10 N3 C11 105.3(4) . . ? C10 N3 Cu 111.3(3) . . ? C11 N3 Cu 143.1(3) . . ? C2 N4 C8 107.7(4) . . ? C2 N5 C3 104.7(4) . . ? C2 N5 Cu 110.9(3) . . ? C3 N5 Cu 143.0(3) . . ? C18 N6 C19 105.6(4) . . ? C18 N6 Cu 112.0(3) . . ? C19 N6 Cu 142.1(3) . . ? C18 N7 C24 107.8(4) . . ? C25 N8 Cu 175.2(4) . . ? N8 Cu N6 98.84(15) . . ? N8 Cu N3 99.10(15) . . ? N6 Cu N3 117.36(14) . . ? N8 Cu N5 98.42(15) . . ? N6 Cu N5 120.09(15) . . ? N3 Cu N5 115.68(14) . . ? N8 Cu N1 179.60(16) . . ? N6 Cu N1 81.14(14) . . ? N3 Cu N1 81.25(14) . . ? N5 Cu N1 81.26(14) . . ? F4 B1 F2 110.9(4) . . ? F4 B1 F3 109.2(4) . . ? F2 B1 F3 109.0(5) . . ? F4 B1 F1 110.0(5) . . ? F2 B1 F1 109.3(4) . . ? F3 B1 F1 108.4(4) . . ? F5' B2 F8 123.7(14) . . ? F7 B2 F8 110.5(8) . . ? F5' B2 F6 113.8(13) . . ? F7 B2 F6 112.1(10) . . ? F8 B2 F6 111.3(4) . . ? F5' B2 F7' 106.0(14) . . ? F8 B2 F7' 99.3(17) . . ? F6 B2 F7' 97.9(14) . . ? F7 B2 F5 109.4(8) . . ? F8 B2 F5 105.5(10) . . ? F6 B2 F5 107.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N5 15.5(6) . . . . ? N1 C1 C2 N4 -167.7(4) . . . . ? C8 C3 C4 C5 1.3(7) . . . . ? N5 C3 C4 C5 -178.4(4) . . . . ? C3 C4 C5 C6 -1.2(7) . . . . ? C4 C5 C6 C7 0.7(8) . . . . ? C5 C6 C7 C8 -0.3(7) . . . . ? C6 C7 C8 C3 0.4(7) . . . . ? C6 C7 C8 N4 178.1(5) . . . . ? N5 C3 C8 C7 178.8(4) . . . . ? C4 C3 C8 C7 -1.0(7) . . . . ? N5 C3 C8 N4 0.6(5) . . . . ? C4 C3 C8 N4 -179.2(4) . . . . ? N1 C9 C10 N3 23.5(5) . . . . ? N1 C9 C10 N2 -160.4(4) . . . . ? C16 C11 C12 C13 -0.7(7) . . . . ? N3 C11 C12 C13 178.5(4) . . . . ? C11 C12 C13 C14 0.1(7) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C12 C11 C16 N2 179.4(4) . . . . ? N3 C11 C16 N2 0.0(5) . . . . ? C12 C11 C16 C15 1.5(7) . . . . ? N3 C11 C16 C15 -177.9(4) . . . . ? N1 C17 C18 N6 23.7(5) . . . . ? N1 C17 C18 N7 -158.0(4) . . . . ? N6 C19 C20 C21 179.3(4) . . . . ? C24 C19 C20 C21 -0.1(6) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? C20 C21 C22 C23 0.8(7) . . . . ? C21 C22 C23 C24 -0.9(7) . . . . ? C22 C23 C24 N7 -178.3(5) . . . . ? C22 C23 C24 C19 0.6(7) . . . . ? C20 C19 C24 N7 179.1(4) . . . . ? N6 C19 C24 N7 -0.4(5) . . . . ? C20 C19 C24 C23 -0.1(7) . . . . ? N6 C19 C24 C23 -179.6(4) . . . . ? C13 C14 C15 C16 1.0(7) . . . . ? N2 C16 C15 C14 -178.9(5) . . . . ? C11 C16 C15 C14 -1.6(7) . . . . ? C2 C1 N1 C17 88.0(4) . . . . ? C2 C1 N1 C9 -147.9(3) . . . . ? C2 C1 N1 Cu -30.3(4) . . . . ? C18 C17 N1 C1 -154.0(3) . . . . ? C18 C17 N1 C9 82.1(4) . . . . ? C18 C17 N1 Cu -35.2(4) . . . . ? C10 C9 N1 C1 82.8(4) . . . . ? C10 C9 N1 C17 -152.8(3) . . . . ? C10 C9 N1 Cu -35.3(4) . . . . ? N3 C10 N2 C16 0.3(5) . . . . ? C9 C10 N2 C16 -176.0(4) . . . . ? C15 C16 N2 C10 177.4(5) . . . . ? C11 C16 N2 C10 -0.2(5) . . . . ? N2 C10 N3 C11 -0.3(5) . . . . ? C9 C10 N3 C11 176.3(4) . . . . ? N2 C10 N3 Cu -175.1(3) . . . . ? C9 C10 N3 Cu 1.5(5) . . . . ? C12 C11 N3 C10 -179.1(5) . . . . ? C16 C11 N3 C10 0.2(5) . . . . ? C12 C11 N3 Cu -7.2(8) . . . . ? C16 C11 N3 Cu 172.1(4) . . . . ? N5 C2 N4 C8 -0.3(5) . . . . ? C1 C2 N4 C8 -177.4(4) . . . . ? C7 C8 N4 C2 -178.2(5) . . . . ? C3 C8 N4 C2 -0.2(5) . . . . ? N4 C2 N5 C3 0.7(5) . . . . ? C1 C2 N5 C3 177.9(4) . . . . ? N4 C2 N5 Cu -169.1(3) . . . . ? C1 C2 N5 Cu 8.1(5) . . . . ? C8 C3 N5 C2 -0.8(5) . . . . ? C4 C3 N5 C2 179.0(5) . . . . ? C8 C3 N5 Cu 163.2(4) . . . . ? C4 C3 N5 Cu -17.1(8) . . . . ? N7 C18 N6 C19 -1.1(5) . . . . ? C17 C18 N6 C19 177.4(4) . . . . ? N7 C18 N6 Cu -177.3(3) . . . . ? C17 C18 N6 Cu 1.3(5) . . . . ? C20 C19 N6 C18 -178.6(5) . . . . ? C24 C19 N6 C18 0.9(5) . . . . ? C20 C19 N6 Cu -4.3(8) . . . . ? C24 C19 N6 Cu 175.2(4) . . . . ? N6 C18 N7 C24 0.9(5) . . . . ? C17 C18 N7 C24 -177.6(4) . . . . ? C23 C24 N7 C18 178.8(5) . . . . ? C19 C24 N7 C18 -0.2(5) . . . . ? _refine_diff_density_max 1.834 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.098 _shelxl_version_number 2012-9